CN105665698B - A kind of method on nano magnalium spinelle presoma resin modified metal aluminium powder surface - Google Patents
A kind of method on nano magnalium spinelle presoma resin modified metal aluminium powder surface Download PDFInfo
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- CN105665698B CN105665698B CN201510748216.0A CN201510748216A CN105665698B CN 105665698 B CN105665698 B CN 105665698B CN 201510748216 A CN201510748216 A CN 201510748216A CN 105665698 B CN105665698 B CN 105665698B
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- aluminium powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a kind of method on nano magnalium spinelle presoma resin modified metal aluminium powder surface, first using aluminium salt and magnesium salts as primary raw material, citric acid is used as complexing agent, and baking oven is put into after being neutrality with ammoniacal liquor regulation pH value, 12 48h are heated at 60 80 DEG C, form magnesium aluminate spinel colloidal sol；Metallic aluminium after purification is put into magnesium aluminate spinel colloidal sol, filtered through ultrasonic disperse, obtains the metallic aluminium powder that surface is wrapped up by magnesium aluminate spinel colloidal sol, is dried 24 36 hours at 80 110 DEG C, obtains the metallic aluminium powder of nano magnalium spinelle modification；The aluminium powder modified by nano magnalium spinelle is put into ethanol phenolic aldehyde liquid after the 10min of ultrasonic disperse 5 again, filtered, 120 150 DEG C of 12 24h of drying, that is, obtains the metallic aluminium powder of nano magnalium spinelle precursor resin parcel；Its hydration resistance is remarkably improved to the modification on metallic aluminium powder surface, after 100 DEG C of aquations are tested 10 hours, anhydrous product occurs；The method of this modified metal aluminium powder, cost is low, and technique is simple, is advantageously implemented industrialization.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, is related to a kind of method that active metal surface is modified, especially
It is related to a kind of method on nano magnalium spinelle presoma-resin modified metal aluminium powder surface.
Technical background
Metallic aluminium powder has a wide range of applications in the industrial production.In fire resisting material field, metallic aluminium powder is commonly used for antioxygen
Agent, and introducing metallic aluminium powder, silica flour make it be formed in situ Non oxide bonded mutually to improve material in carbon composite of shaping
The high-temperature behavior of material is the new focus that fire resisting material field was studied in recent years, and achieves preferable effect.But for unsetting
Carbon composite, such as carbon containing castable, due to the easy aquation of metallic aluminium powder, limit its application in unshape refractory.
And unshape refractory has energy-conserving and environment-protective, technique is simple, remarkable in economical benefits, and is easy to construct in complex-shaped region
The advantages that.In developed country, the ratio of unshape refractory has accounted for more than 60%, and Japan is up to 75% or so, and China is unsetting
Refractory material proportion averagely about 35% or so, there is very big development space.Therefore, to widen metallic aluminium powder applies model
Enclose, it is applied successfully in unshape refractory, research and develop high performance indefinite refractory material, it is anti-must just to improve it
Hydrability, the modification on metallic aluminium powder surface are very crucial.In addition, granularity it is thinner metallic aluminium powder surface it is oxidizable, so as to
Influence the performance of its performance.Therefore, it is surface modified to metallic aluminium powder, its hydration resistance can be not only improved, may also suppress
The oxidation on its surface.
At present, about research surface modified metal Al mainly with unitary oxide sol（Alumina gel, Ludox）
To be surface-treated（Jia Quanli, Ye Fangbao, Zhang Yucui, Zhong Xiangchong；A kind of surface treatment side for improving hydration resistance of aluminum powder
Method；The patent No.：ZL 201110198043.1.Sasaki, T., Aida, H., Niizaki, T. and Abe, M.
(1998) Coated Aluminum Powder for Additive of Castable Refractory, Japanese
Patent, 10-7931.Liu Yaopeng, Yang Yi；Nano-meter SiO_22The preparation of/Al compound particles；Chemical industry is in progress, and 2005,24（2）：
178-181）, the diaphragm of one layer of presoma containing nanometer and then the hydration resistance of raising aluminium are formed on aluminium powder surface, and before nanometer
Drive body and form nano-particle at high temperature, the high-temperature behavior of refractory material can be improved.However, the Alumina gel on aluminium powder surface, silicon are molten
When glue drying becomes gel, easily forming blind crack causes hydration resistance of aluminum powder to reduce, and the gel and aluminum substrate on aluminium powder surface
Bond strength is not high, and the action face decorative layer in practical application by frictional force is easy to fall off, exposes aluminium and comes, therefore, this
Certain defect be present in the method that kind improves hydration resistance of aluminum powder.
The content of the invention
To solve the easy aquation of metallic aluminium powder, restricted technical problem, Yi Jijin being used in aqueous refractory material system
The problem of surface is oxidizable when belonging to the storage of aluminium powder normal temperature, the present invention provide a kind of metallic aluminium powder surface modified one kind side
Method, and the metallic aluminium powder with excellent hydration resistance is prepared, to widen the application field of metallic aluminium powder.
The technical scheme is that realize in the following manner：
A kind of method on nano magnalium spinelle presoma-resin modified metal aluminium powder surface,（One）, first with aluminium salt and magnesium
Salt is primary raw material, uses citric acid as complexing agent, and pH value is adjusted with ammoniacal liquor；First aluminium salt and magnesium salts are dissolved in distilled water,
Add citric acid and make complexing agent, the wherein mol ratio of aluminium salt, magnesium salts and citric acid is 2:1:0.2, then add appropriate ammoniacal liquor and adjust
The pH value for saving solution is neutrality, is put into baking oven after this neutral solution is well mixed, 12-48h is heated at 60-80 DEG C, with shape
Into magnesium aluminate spinel colloidal sol；（Two）, metallic aluminium powder after purification is put into magnesium aluminate spinel colloidal sol, metallic aluminium powder and magnalium point
Spar sol weight ratio is 1:Filtered after 5, ultrasonic disperse 3-5min, obtain the metallic aluminium that surface is wrapped up by magnesium aluminate spinel colloidal sol
Powder, 24-36 hours are dried at 80-110 DEG C, obtain the metallic aluminium powder of nano magnalium spinelle presoma modification；（Three）By nothing
Water-ethanol is incorporated into thermosetting phenolic resin and is well mixed, and the weight ratio of absolute ethyl alcohol and resin is 1:2, then will be by nanometer Mg
Aluminate presoma modification aluminium powder be put into ethanol-phenolic aldehyde liquid, nano magnalium spinelle presoma modification aluminium powder with
The weight ratio of ethanol-phenolic aldehyde liquid is 1:After 10, ultrasonic disperse 5-10min, filter, 120-150 DEG C of dry 12-24h, that is, received
The metallic aluminium powder of rice magnesium aluminate spinel presoma-resin modification；
Described aluminium salt is the one or more in aluminum nitrate, aluminium chloride, aluminum sulfate；
Described magnesium salts is the one or more in magnesium nitrate, magnesium chloride, magnesium sulfate.
The granularity of described metallic aluminium powder is 40-80 microns, and purity is more than 99.5%.
During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 60 DEG C, heat time 48h.
During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 70 DEG C, heat time 28h.
During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 80 DEG C, heat time 12h.
It is described obtain the metallic aluminium powder of nano magnalium spinelle presoma modification during, drying temperature is 80 DEG C,
Drying time is 36 hours.
During the described metallic aluminium powder for obtaining nano magnalium spinelle presoma and modifying, drying temperature 110
DEG C, drying time be 24 hours.
It is described obtain the metallic aluminium powder of nano magnalium spinelle presoma modification during, drying temperature is 90 DEG C,
Drying time is 28 hours.
It is described the aluminium powder modified by nano magnalium spinelle presoma is put into ethanol-phenolic aldehyde liquid again during,
Drying temperature is 120 DEG C, drying time 24h.
Described is again put into the aluminium powder modified by nano magnalium spinelle presoma in ethanol-phenolic aldehyde liquid process, does
Dry temperature is 150 DEG C, drying time 12h.
The technological merit of the present invention is：
（1）Its hydration resistance can be improved to the modification on metallic aluminium powder surface, using nano magnalium spinelle forerunner
Body-resin is modified metallic aluminium powder surface, can not only improve the hydration resistance of metallic aluminium, the nano magnalium of metallic aluminum surface
Spinelle presoma forms nano particle at high temperature, has activeness and quietness effect to refractory material, can also improve the anti-of material
Aggressivity.And magnesium aluminate spinel belongs to binary oxide, it is than unitary oxide（Such as：Aluminum oxide, silica）With more excellent
Good high-temperature behavior.
（2）Can shape come modified metal aluminium powder, metallic aluminium powder surface using nano magnalium spinelle presoma and phenolic resin
Into firm inorganic-organic hybrid coating film, the consistency of finishing coat and the bond strength with aluminum substrate can be improved,
Finishing coat is not fallen off when being acted on by frictional force, and then improves the hydration resistance of aluminium powder.
（3）The method has technique simple, and cost is low, and metallic aluminium hydration resistance is good, after 100 DEG C of aquations are tested 10 hours,
Anhydrous product occurs.
Brief description of the drawings
Fig. 1 is the thing phase composition schematic diagram after the aquations experiment 10 hours of 100 DEG C of Al powder after modifying.
Embodiment
With reference to embodiment, the invention will be further described, but is not limited to the following example.
Embodiment 1
Raw material, aluminum nitrate are weighed in molar ratio：Magnesium nitrate：Citric acid=2:1:0.2, first by 426g aluminum nitrates and 148g nitre
Sour magnesium is dissolved in 1000 milliliters of distilled water, is stirred with glass bar untill powder all dissolving.Then 38.4g lemons are added
Acid, stirred with glass bar to being completely dissolved, form clear solution.Ammoniacal liquor is slowly added into rubber head dropper again above-mentioned transparent molten
Xie Zhong, the pH value of solution is determined with PH test paper, until the pH value of solution is 7.
The above-mentioned solution for mixing up pH value is put into baking oven, 48h is heated at 60 DEG C, to form magnesium aluminate spinel colloidal sol.
40 micron metal aluminium powder 15g after purification are put into 75g magnesium aluminate spinel colloidal sols, is filtered after ultrasonic disperse 3min, obtains table
Face obtains surface by nano magnalium spinelle by the metallic aluminium powder of magnesium aluminate spinel Sol-Modified after being dried 36 hours at 80 DEG C
The metallic aluminium powder of presoma modification.
150g absolute ethyl alcohols are incorporated into 300g thermosetting phenolic resins and are well mixed, then will be by nano magnalium spinelle
The aluminium powder 20g of presoma modification is put into 200g ethanol-phenolic resin liquid, after ultrasonic disperse 5min, is filtered, 120 DEG C of dryings
24h.
Embodiment 2
Raw material, aluminum nitrate are weighed in molar ratio：Magnesium nitrate：Citric acid=2:1:0.2, first by 426g aluminum nitrates and 148g nitre
Sour magnesium is dissolved in 1000 milliliters of distilled water, is stirred to powder with glass bar and is all dissolved in distilled water.Then 38.4g is added
Citric acid, stirred with glass bar to being completely dissolved, form clear solution.Ammoniacal liquor is slowly added into rubber head dropper again above-mentioned
In bright dissolving, the pH value of solution is determined with PH test paper, until the pH value of solution is 7.
The above-mentioned solution for mixing up pH value is put into baking oven, 36h is heated at 70 DEG C, with the magnalium formed with certain viscosity
Spinelle colloidal sol.60 micron metal aluminium powder 15g after purification are put into 75g magnesium aluminate spinel colloidal sols, after ultrasonic disperse 3min
Filter, obtain surface by the metallic aluminium powder of magnesium aluminate spinel Sol-Modified, obtaining surface after being dried 30 hours at 90 DEG C is received
The metallic aluminium powder of rice magnesium aluminate spinel presoma modification.
150g absolute ethyl alcohols are incorporated into 300g thermosetting phenolic resins and are well mixed, then will be by nano magnalium spinelle
The aluminium powder 20g of presoma modification is put into 200g ethanol-phenolic resin liquid, after ultrasonic disperse 4min, is filtered, 130 DEG C of dryings
18h.
Embodiment 3
Raw material, aluminium chloride are weighed in molar ratio：Magnesium chloride：Citric acid=2:1:0.2, first by 266.4g aluminium chloride and 94.8g
Magnesium chloride is dissolved in 1000 milliliters of distilled water, is stirred to whole and is dissolved in distilled water with glass bar.Then citric acid is added, is used
Glass bar is stirred to being completely dissolved, and forms clear solution.Ammoniacal liquor is slowly added into above-mentioned transparent dissolving with rubber head dropper again,
The pH value of solution is determined with PH test paper, until the pH value of solution is 7.
The above-mentioned solution for mixing up pH value is put into baking oven, 12h is heated at 80 DEG C, with the magnalium formed with certain viscosity
Spinelle colloidal sol.80 micron metal aluminium powder 15g after purification are put into 75g magnesium aluminate spinel colloidal sols, taken out after ultrasonic disperse 5min
Filter, surface is obtained by the metallic aluminium of magnesium aluminate spinel Sol-Modified, surface is obtained by nanometer Mg after being dried 24 hours at 110 DEG C
The metallic aluminium powder of aluminate presoma modification.
150g absolute ethyl alcohols are incorporated into 300g thermosetting phenolic resins and are well mixed, then will be by nano magnalium spinelle
The aluminium powder 20g of presoma modification is put into 200g ethanol-phenolic resin liquid, after ultrasonic disperse 10min, is filtered, and 150 DEG C dry
Dry 12h.
Embodiment 4
Raw material, aluminum sulfate are weighed in molar ratio：Magnesium sulfate：Citric acid=2:1:0.2, first by 684g aluminum sulfate and 120g sulphur
Sour magnesium is dissolved in 1000 milliliters of distilled water, is stirred to whole and is dissolved in distilled water with glass bar.Then 38.4g lemons are added
Acid, stirred with glass bar to being completely dissolved, form clear solution.Ammoniacal liquor is slowly added into rubber head dropper again above-mentioned transparent molten
Xie Zhong, the pH value of solution is determined with PH test paper, until the pH value of solution is 7.
The above-mentioned solution for mixing up pH value is put into baking oven, 36h is heated at 70 DEG C, with the magnalium formed with certain viscosity
Spinelle colloidal sol.70 micron metal aluminium powder 15g after purification are put into 75g magnesium aluminate spinel colloidal sols, after ultrasonic disperse 4min
Filter, obtain surface by the metallic aluminium of magnesium aluminate spinel Sol-Modified, surface is obtained by nanometer after being dried 30 hours at 100 DEG C
The metallic aluminium powder of magnesium aluminate spinel presoma modification.
150g absolute ethyl alcohols are incorporated into 300g thermosetting phenolic resins and are well mixed, then will be by nano magnalium spinelle
The aluminium powder 20g of presoma modification is put into 300g ethanol-phenolic resin liquid, after ultrasonic disperse 8min, is filtered, 140 DEG C of dryings
15h.
Embodiment 5
Raw material, aluminum nitrate are weighed in molar ratio：Magnesium chloride：Citric acid=2:1:0.2, first by 426g aluminum nitrates and 94.8g chlorine
Change magnesium to be dissolved in 1000 milliliters of distilled water, stirred to whole and be dissolved in distilled water with glass bar.Then 38.4g lemons are added
Acid, stirred with glass bar to being completely dissolved, form clear solution.Ammoniacal liquor is slowly added into rubber head dropper again above-mentioned transparent molten
Xie Zhong, the pH value of solution is determined with PH test paper, until the pH value of solution is 7.
The above-mentioned solution for mixing up pH value is put into baking oven, 33h is heated at 75 DEG C, with the magnalium formed with certain viscosity
Spinelle colloidal sol.60 micron metal aluminium powder 15g after purification are put into 75g magnesium aluminate spinel colloidal sols, ultrasonic disperse 3.5min
After filter, obtain surface by the metallic aluminium of magnesium aluminate spinel Sol-Modified, obtaining surface after being dried 30 hours at 100 DEG C is received
The metallic aluminium powder of rice magnesium aluminate spinel presoma modification.
Appropriate absolute ethyl alcohol 150g is incorporated into 300g thermosetting phenolic resins and is well mixed, then will be by nano magnalium point
The aluminium powder 20g of spar presoma modification is put into 200g ethanol-phenolic resin liquid, after ultrasonic disperse 6min, is filtered, 130 DEG C
Dry 20h.
Fig. 1 shows that aquation only has metal Al peak, anhydrous product Al (OH) after testing3Generation, show metal after modification
Al powder has excellent hydration resistance.
Claims (10)
1. a kind of method on nano magnalium spinelle presoma-resin modified metal aluminium powder surface,（One）, first with aluminium salt and magnesium salts
For primary raw material, citric acid is used as complexing agent, and p H values are adjusted with ammoniacal liquor；First aluminium salt and magnesium salts are dissolved in distilled water, added
Enter citric acid and make complexing agent, the wherein mol ratio of aluminium salt, magnesium salts and citric acid is 2:1:0.2, then add appropriate ammoniacal liquor regulation
The p H values of solution are neutrality, are put into baking oven after this neutral solution is well mixed, 12-48h is heated at 60-80 DEG C, to be formed
Magnesium aluminate spinel colloidal sol；（Two）, metallic aluminium powder after purification is put into magnesium aluminate spinel colloidal sol, metallic aluminium powder and magnalium point are brilliant
Stone sol weight ratio is 1:Filtered after 5, ultrasonic disperse 3-5min, obtain the metallic aluminium that surface is wrapped up by magnesium aluminate spinel colloidal sol
Powder, 24-36 hours are dried at 80-110 DEG C, obtain the metallic aluminium powder of nano magnalium spinelle precursor modification；（Three）By nothing
Water-ethanol is incorporated into thermosetting phenolic resin and is well mixed, and the weight ratio of absolute ethyl alcohol and resin is 1:2, then will be by nanometer Mg
The aluminium powder of aluminate precursor modification is put into ethanol-phenolic aldehyde liquid, the metallic aluminium of nano magnalium spinelle precursor modification
The weight ratio of powder and ethanol-phenolic aldehyde liquid is 1:After 10, ultrasonic disperse 5-10min, filter, 120-150 DEG C of dry 12-24h, i.e.,
Obtain the metallic aluminium powder of nano magnalium spinelle precursor-resin modification；
Described aluminium salt is the one or more in aluminum nitrate, aluminium chloride, aluminum sulfate；
Described magnesium salts is the one or more in magnesium nitrate, magnesium chloride, magnesium sulfate.
2. the method on nano magnalium spinelle presoma according to claim 1-resin modified metal aluminium powder surface, it is special
Sign is：The granularity 40-80 microns of described metallic aluminium powder, purity are more than 99.5%.
3. the method on nano magnalium spinelle presoma according to claim 2-resin modified metal aluminium powder surface, it is special
Sign is：During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 60 DEG C, heat time 48h.
4. the method on nano magnalium spinelle presoma according to claim 2-resin modified metal aluminium powder surface, it is special
Sign is：During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 70 DEG C, heat time 28h.
5. the method on nano magnalium spinelle presoma according to claim 2-resin modified metal aluminium powder surface, it is special
Sign is：During described formation magnesium aluminate spinel colloidal sol, heating-up temperature is 80 DEG C, heat time 12h.
6. according to any described nano magnalium spinelle presoma-resin modified metal aluminium powder surface of claim 2,3,4,5
Method, it is characterised in that：During the described metallic aluminium powder for obtaining nano magnalium spinelle precursor and modifying, temperature is dried
It is 36 hours to spend for 80 DEG C, drying time.
7. according to any described nano magnalium spinelle presoma-resin modified metal aluminium powder surface of claim 2,3,4,5
Method, it is characterised in that：During the described metallic aluminium powder for obtaining nano magnalium spinelle precursor and modifying, temperature is dried
It is 24 hours to spend for 110 DEG C, drying time.
8. according to any described nano magnalium spinelle presoma-resin modified metal aluminium powder surface of claim 2,3,4,5
Method, it is characterised in that：During the described metallic aluminium powder for obtaining nano magnalium spinelle precursor and modifying, temperature is dried
It is 28 hours to spend for 90 DEG C, drying time.
9. the method on nano magnalium spinelle presoma according to claim 8-resin modified metal aluminium powder surface, it is special
Sign is：Described is put into ethanol-phenolic aldehyde liquid by the aluminium powder modified by nano magnalium spinelle precursor again and obtains nanometer
During the metallic aluminium powder of magnesium aluminate spinel precursor-resin modification, drying temperature is 120 DEG C, drying time 24h.
10. the method on nano magnalium spinelle presoma according to claim 8-resin modified metal aluminium powder surface, its
It is characterised by：Described is put into ethanol-phenolic aldehyde liquid by the aluminium powder modified by nano magnalium spinelle precursor again and is received
During the metallic aluminium powder of rice magnesium aluminate spinel precursor-resin modification, drying temperature is 150 DEG C, drying time 12h.
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| CN106876199B (en) * | 2017-01-23 | 2018-10-02 | 西安工程大学 | A kind of preparation method of the siller tin oxide alloy as electric contact material of even tissue |
| CN106807953B (en) * | 2017-01-23 | 2018-07-10 | 西安工程大学 | A kind of preparation method of tin oxide disperse enhancing silver-based electric contact alloy |
| CN110207499A (en) * | 2019-06-20 | 2019-09-06 | 武汉科技大学 | Anode material of lithium battery sintering saggar based on magnesium aluminate spinel colloidal sol and preparation method thereof |
| CN115028455B (en) * | 2022-07-11 | 2023-06-02 | 中钢集团洛阳耐火材料研究院有限公司 | Baking-free silicon carbide-magnesia alumina spinel refractory material, preparation method and product thereof |
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| CN101565194A (en) * | 2009-06-01 | 2009-10-28 | 西北大学 | Method for preparing superfine mesoporous magnesium aluminate spinel |
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| CN101891484A (en) * | 2010-07-16 | 2010-11-24 | 西安电子科技大学 | Method for improving homodisperse of nanometer magnesia-alumina spinel in aluminous fireproof material |
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Granted publication date: 20171110 Termination date: 20181106 |